CN105397085A - Method for preparing nickel-based powder superalloy through spark plasma sintering - Google Patents

Method for preparing nickel-based powder superalloy through spark plasma sintering Download PDF

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CN105397085A
CN105397085A CN201510672555.5A CN201510672555A CN105397085A CN 105397085 A CN105397085 A CN 105397085A CN 201510672555 A CN201510672555 A CN 201510672555A CN 105397085 A CN105397085 A CN 105397085A
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superalloy
powder
base
plasma sintering
nickel
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CN105397085B (en
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刘祖铭
苏鹏飞
麻梦梅
郭旸
段然曦
王帅
辜恩泽
段清龙
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Central South University
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Central South University
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Abstract

The invention discloses a method for preparing nickel-based powder superalloy through spark plasma sintering, and belongs to the field of powder metallurgy materials. The spark plasma sintering process is adopted for sintering forming of atomized nickel-based superalloy powder, and then solid solution treatment and aging treatment are carried out to obtain the nickel-based powder superalloy. The spark plasma sintering process is adopted for preparing the nickel-based powder superalloy, rapid sintering forming of the powder is achieved, growth of grains can be effectively restrained, and the prepared superalloy is provided with the fine and uniform equiaxial structure; through powder surface discharge activation and rapid diffusion bonding, formation of complex carbides and oxides on the boundaries of powder particles is restrained, and original particle boundaries are eliminated; the method is simple in process route, preparation time is short, the second phase is small in size and uniform in distribution, and the mechanical property is good.

Description

A kind of discharge plasma sintering prepares the method for Ni-base P/M Superalloy
Technical field
The present invention relates to a kind of method that discharge plasma sintering prepares Ni-base P/M Superalloy, belong to powdered metallurgical material field.
Background technology
Ni-base P/M Superalloy has that crystal grain is tiny, even tissue, without gross segregation, the feature such as alloying level is high, yield strength is high and fatigue behaviour is excellent, be the preferred material manufacturing advanced engine thermal end pieces.
The preparation of Ni-base P/M Superalloy mainly comprises two technology paths, and one is the countries such as America and Europe, main employing " argon gas atomization (AA) powder hot extrusion (HEX) shaping+isothermal forging (ITF) " preparation technology; Two is the countries such as Russia, main employing " the direct high temperature insostatic pressing (HIP) of plasma rotating electrode (PREP) powder (As-HIP) shaping " preparation technology.
P & WA company of the U.S. is first in 1972, argon gas powder by atomization+hot extrusion+isothermal forging process is adopted to prepare IN100 powder metallurgy superalloy, as 11 kinds of parts such as compressor disc and the turbine disk of F100 engine, direct heat and other static pressuring processes within 1976, is adopted to have developed the LCAstroloy powder turbine disk, for JT8D-17R and TF-30 engine.The TF/A-18 aircraft low-pressure turbine dish that a frame in 1980 is equipped with F404 engine breaks after accident, and the manufacturing process of the U.S. to powder disk adjusts, and adopts high temperature insostatic pressing (HIP)/hot extrusion+isothermal forging process to prepare the powder turbine disk.
China starts in 20 century 70s the research carrying out powder metallurgy superalloy, prepares to two kinds of techniques the research work that powder metallurgy superalloy is all correlated with.Chinese patent CN102392147A, disclose a kind of ultrafine grain nickel base powder high temperature alloy preparation method, plasma rotating electrode process or Powder In Argon Atomization is adopted to prepare superalloy powder, dense powder high temperature alloy blank is obtained through Powder hot isostatic pressure, then the coated blank of non-metallic insulation material is used, again coated good ingot blank is carried out the accurate isothermal forging that forging and stamping pier slightly controls with local deformation to combine, obtain biscuit.Finally, the biscuit of forging is carried out recrystallization annealing process, acquisition even tissue, the powder metallurgy superalloy biscuit that crystal grain is tiny.Chinese patent CN104493167A, provide a kind of thermal extrusion moulding method of powder metallurgy superalloy annular element, argon gas will be adopted to be atomized superalloy powder and to load hot extrusion annular sheath, first high temperature insostatic pressing (HIP) obtains ingot blank, then carry out large extrusion ratio (10 ~ 20) hot extrusion to ingot blank, machining goes out sheath material to obtain powder metallurgy superalloy.
Current employing high temperature insostatic pressing (HIP) or hot extrusion+isothermal forging are shaped and prepare Ni-base P/M Superalloy technological process complexity, and length consuming time, preparation cost is high.Adopt high temperature insostatic pressing (HIP) to be shaped and prepare powder metallurgy superalloy, because temperature retention time is longer, crystal grain is easily grown up, and the active element of oxygen easily and in alloy of powder surface absorption reacts, form oxide on powder particle border, cause occurring primary granule border, fall low-alloyed mechanical property.
For above-mentioned Problems existing, this patent proposes discharge plasma sintering process and prepares Ni-base P/M Superalloy.
Summary of the invention
A kind of discharge plasma sintering is the object of the present invention is to provide to prepare the method for Ni-base P/M Superalloy.
A kind of discharge plasma sintering of the present invention prepares the method for Ni-base P/M Superalloy, with nickel-base high-temperature powder for raw material, through solid solution and Ageing Treatment after being shaped, obtains Ni-base P/M Superalloy by discharge plasma sintering.
A kind of discharge plasma sintering of the present invention prepares the method for Ni-base P/M Superalloy, and described nickel-base high-temperature powder is argon gas atomization Ni-base Superalloy Powder.
A kind of discharge plasma sintering of the present invention prepares the method for Ni-base P/M Superalloy, and the granularity of described nickel-base high-temperature powder is less than or equal to 75 μm.
A kind of discharge plasma sintering of the present invention prepares the method for Ni-base P/M Superalloy, and the technological parameter that discharge plasma sintering is shaped is: temperature 1000 ~ 1200 DEG C, pressure 40 ~ 100MPa; Temperature retention time 5 ~ 20min.
A kind of discharge plasma sintering of the present invention prepares the method for Ni-base P/M Superalloy, and the temperature of described solution treatment is 1000 ~ 1250 DEG C, temperature retention time 1 ~ 2h.
A kind of discharge plasma sintering of the present invention prepares the method for Ni-base P/M Superalloy, and the temperature of Ageing Treatment is 700 ~ 900 DEG C, temperature retention time 4 ~ 10h.
Advantage of the present invention and good effect:
The present invention proposes to adopt discharge plasma sintering to prepare Ni-base P/M Superalloy, has the following advantages and good effect:
The first, discharge plasma sintering prepares Ni-base P/M Superalloy, and can realize powder Fast Sintering and be shaped, effectively suppress growing up of crystal grain, the alloy of preparation has tiny, uniform equiaxed grain structure.
Second, discharge plasma sintering is adopted to prepare Ni-base P/M Superalloy, be connected with rapid diffusion by powder particle surface discharge activation, being rapidly heated and the combination of powder metallurgical interface of powder surface can be realized, suppress the formation of powder particle complex boundary carbide, oxide, eliminate primary granule border.
3rd, adopt discharge plasma sintering to prepare Ni-base P/M Superalloy, process route is simple, and preparation time is short, and second-phase size is tiny, be evenly distributed, good mechanical performance.
In sum, the present invention is a kind of method preparing Ni-base P/M Superalloy fast, and the method effectively can control grain growth, eliminate primary granule border, improves mechanical property.
Accompanying drawing explanation
Accompanying drawing 1 is microscopic structure ESEM (SEM) figure of the nickel base superalloy of the hot-pressed preparation of comparative example 1 atomized powder 1150 DEG C of large extrusion ratios (10:1);
Accompanying drawing 2 is comparative example 2 [documents: Zhao Junpu, Tao Yu, Yuan Shouqian, Deng. primary granule border (PPB) problem [J] in powder metallurgy high-temperature alloy. powder metallurgy industry, 2010 (04): 43-49] atomized powder high temperature insostatic pressing (HIP) is shaped the microscopic structure of nickel base superalloy of preparation.
Accompanying drawing 3 is microscopic structure ESEM (SEM) figure of the nickel base superalloy of embodiment 1 atomized powder 1150 DEG C of plasma agglomerations shaping preparations.
Accompanying drawing 4 is microscopic structures of the Ni-base P/M Superalloy of embodiment 1 atomized powder 1150 DEG C of plasma agglomerations shaping preparations.The alloy phase ratio prepared with accompanying drawing 2 high temperature insostatic pressing (HIP), primary granule border is eliminated substantially.
The grain size number can finding out gained nickel base superalloy from accompanying drawing 1 is ASTM9 level, and crystal grain is thicker.
In accompanying drawing 2,1,2,3 borders representing primary granule respectively.As can be seen from accompanying drawing 2, the microscopic structure of the nickel base superalloy of comparative example 2 atomized powder high temperature insostatic pressing (HIP) shaping preparation can observe obvious primary granule border, as 1, and 2, shown in 3.
As can be seen from accompanying drawing 3, the second-phase of embodiment 1 gained finished product is evenly distributed, and crystal grain is tiny, even, and grain size number is ASTM10 level, and the alloy grain comparing the hot-pressed preparation shown in accompanying drawing 1 is more tiny, even.
As can be seen from accompanying drawing 4, in the finished product prepared by embodiment 1, its primary granule border obviously disappears, and after contrasting with accompanying drawing 2, this sign is just more obvious.
Detailed description of the invention
Below in conjunction with accompanying drawing and concrete comparative example and embodiment, the invention will be further described.
Comparative example 1:
Argon gas is atomized Ni-based pre-alloyed powder (composition is Ni-20.6Co-13Cr-3.8Mo-2.1W-3.4Al-3.9Ti-2.4Ta-0.9Nb (wt%)) and loads steel capsule, vacuumize degasification, sealing; Carry out hot-pressed at 1150 DEG C, extrusion ratio is 10:1, obtains nickel-base alloy bar; Last at 1180 DEG C of solid solution 1h, 815 DEG C of timeliness 8h, obtain nickel base superalloy.
The room-temperature mechanical property of alloy is: fracture strength 1197MPa, yield strength 827MPa, percentage elongation 4.94%, density 8.1787g/cm 3.The microscopic structure of alloy is shown in accompanying drawing 1, and grain size number is ASTM9 level.
Comparative example 2: document [Zhao Junpu, Tao Yu, Yuan Shouqian, etc. primary granule border (PPB) problem [J] in powder metallurgy high-temperature alloy. powder metallurgy industry, 2010 (04): 43-49]
Argon gas is atomized Ni-based pre-alloyed powder (composition is Ni-13Co-16Cr-4Mo-4W-2.2Al-3.7Ti-0.8Nb (wt%)) and loads steel capsule, vacuumize degasification, sealing; Carry out high temperature insostatic pressing (HIP) shaping at 1180 DEG C/130MPa, the time is 3h, obtains nickel-base alloy blank.The microscopic structure of alloy is shown in accompanying drawing 2, has occurred obvious primary granule border.
Comparative example 3
Argon gas is atomized Ni-based pre-alloyed powder (composition is Ni-20.6Co-13Cr-3.8Mo-2.1W-3.4Al-3.9Ti-2.4Ta-0.9Nb (wt%)) and carries out plasma agglomeration at 900 DEG C/40MPa, insulation 20min, then solution treatment is carried out: 900 DEG C/3h, then Ageing Treatment is carried out: 700 DEG C/8h, obtain nickel base superalloy.
The room-temperature mechanical property of alloy is: fracture strength 57MPa, and material becomes fragility; Density 7.0g/cm 3.
Embodiment 1:
Argon gas is atomized Ni-based pre-alloyed powder (composition is Ni-20.6Co-13Cr-3.8Mo-2.1W-3.4Al-3.9Ti-2.4Ta-0.9Nb (wt%)) and carries out plasma agglomeration at 1150 DEG C/40MPa, insulation 5min, prepares blank; Then solution treatment is carried out: 1180 DEG C/1h, Ageing Treatment: 815 DEG C/8h, obtain nickel base superalloy.
The room-temperature mechanical property of alloy is: fracture strength 1273MPa; Yield strength 906MPa; Percentage elongation 10.65%; Density 8.1735g/cm 3.The microscopic structure of alloy is shown in accompanying drawing 3,4, and grain size number is ASTM10 level, and primary granule border is eliminated substantially.
Embodiment 2:
Argon gas is atomized Ni-based pre-alloyed powder (composition is Ni-20.6Co-13Cr-3.8Mo-2.1W-3.4Al-3.9Ti-2.4Ta-0.9Nb (wt%)) and carries out plasma agglomeration at 1100 DEG C/60MPa, insulation 10min, prepares blank; Then solution treatment is carried out: 1115 DEG C/1h+1170 DEG C/3h, Ageing Treatment: 845 DEG C/8h+760 DEG C/8h, obtain nickel base superalloy.

Claims (6)

1. discharge plasma sintering prepares a method for Ni-base P/M Superalloy, it is characterized in that: with nickel-base high-temperature powder for raw material, through solution treatment and Ageing Treatment after shaping by discharge plasma sintering, obtains Ni-base P/M Superalloy.
2. discharge plasma sintering according to claim 1 prepares the method for Ni-base P/M Superalloy, it is characterized in that: described nickel-base high-temperature powder is argon gas atomization Ni-base Superalloy Powder.
3. discharge plasma sintering according to claim 1 prepares the method for Ni-base P/M Superalloy, it is characterized in that: the granularity of described nickel-base high-temperature powder is less than or equal to 75 μm.
4. the discharge plasma sintering according to claims 1 to 3 any one prepares the method for Ni-base P/M Superalloy, it is characterized in that; The technological parameter that discharge plasma sintering is shaped is: temperature 1000 ~ 1200 DEG C, pressure 40 ~ 100MPa, temperature retention time 5 ~ 20min.
5. discharge plasma sintering according to claim 1 prepares the method for Ni-base P/M Superalloy, it is characterized in that; The temperature of described solution treatment is 1000 ~ 1250 DEG C, temperature retention time 1 ~ 2h.
6. discharge plasma sintering according to claim 1 prepares the method for Ni-base P/M Superalloy, it is characterized in that; The temperature of Ageing Treatment is 700 ~ 900 DEG C, temperature retention time 4 ~ 10h.
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CN107457404A (en) * 2017-08-02 2017-12-12 华中科技大学 A kind of increasing material suitable for complicated part and mould shapes method
CN108405848A (en) * 2018-02-06 2018-08-17 西南交通大学 A kind of porous nickel framework material and preparation method thereof
CN110340350A (en) * 2019-08-27 2019-10-18 湖南伊澍智能制造有限公司 A kind of nickel-base composite material and its preparation method and application
CN111304476A (en) * 2020-02-29 2020-06-19 郑州航空工业管理学院 Preparation method of fine-grain powder superalloy for inhibiting formation of original grain boundary
CN112008087A (en) * 2020-08-30 2020-12-01 中南大学 Method for improving comprehensive performance of carbon nano material reinforced nickel-based high-temperature alloy
CN112063894A (en) * 2020-08-13 2020-12-11 中南大学 Method for preparing precipitation-strengthened high-entropy alloy by spark plasma sintering
CN113134608A (en) * 2021-03-30 2021-07-20 北京航空航天大学 Device and method for preparing nickel-based high-temperature alloy blank by pulse current auxiliary sintering

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Publication number Priority date Publication date Assignee Title
CN107457404A (en) * 2017-08-02 2017-12-12 华中科技大学 A kind of increasing material suitable for complicated part and mould shapes method
CN107457404B (en) * 2017-08-02 2021-01-05 华中科技大学 Additive machining forming method suitable for complex parts and dies
CN108405848A (en) * 2018-02-06 2018-08-17 西南交通大学 A kind of porous nickel framework material and preparation method thereof
CN110340350A (en) * 2019-08-27 2019-10-18 湖南伊澍智能制造有限公司 A kind of nickel-base composite material and its preparation method and application
CN111304476A (en) * 2020-02-29 2020-06-19 郑州航空工业管理学院 Preparation method of fine-grain powder superalloy for inhibiting formation of original grain boundary
CN112063894A (en) * 2020-08-13 2020-12-11 中南大学 Method for preparing precipitation-strengthened high-entropy alloy by spark plasma sintering
CN112063894B (en) * 2020-08-13 2022-02-01 中南大学 Method for preparing precipitation-strengthened high-entropy alloy by spark plasma sintering
CN112008087A (en) * 2020-08-30 2020-12-01 中南大学 Method for improving comprehensive performance of carbon nano material reinforced nickel-based high-temperature alloy
CN113134608A (en) * 2021-03-30 2021-07-20 北京航空航天大学 Device and method for preparing nickel-based high-temperature alloy blank by pulse current auxiliary sintering

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